冰川棘豆生物碱的提取分离

将冰川棘豆阴干 ,粉碎 ,过 2 0目筛。用 15倍量MeOH冷渗 ,减压回收溶剂 ,浓缩物加 0 1mol/LHCl溶解 ,过夜 ,过滤 ,酸水液以 80 0～ 10 0 0ml/ (min·cm2 )流经H+ 阳离子交换树脂。树脂出柱 ,水洗去悬浮物 ,上柱继续洗至无色 ,改用Me2 CO洗至流出液遇NH3 ·H2 O不变色后 ,将树脂倒入烧杯中 ,加 2mol/LNH3 ·H2 O适量 ,密闭 30min ,挥去NH3 ·H2 O ,再上柱 ,Me2 CO洗脱 ,回收溶剂得粗提物 ,粗提物用 1%HCl溶解 ,CHCl3 振摇洗涤数次 ,酸水层调pH 10 ,CHCl3 萃取 ,减压回收溶剂得粗碱 ,用石油醚溶出总碱 ,经硅胶G(含微量NaOH)柱层析 ,CHCl3 Me2 CO恒沸物洗脱 ,每 10ml收 1份 ,TLC检查 ,同类合并 ,石油醚重结晶 ,得晶Ⅰ和晶Ⅱ。并对它们的理化特性进行了初步测定。

Extraction and Separation of Alkaloids from Glacial Crazyweed (Oxytropis glacialis)

The samples of glacial crazyweed (Oxytropis glacialis Benth ex bye) at the stage of flower and pod were collected from Ali prefecture of Xizang (Tibet) autonomous region,identified by Northern Plateau Biological Institute.The samples were dried by air,ground to a 20-mesh powder,and stored in plastic bags at room temperature until used.The crude extract of O.glacialis with methanol was redissolved with 0.1 mol/L hydrochloric acid,filtered.The acid soluble portion was given to a strong cation-exchange resin column,after eluting with water and acetone,the resin was ammoniated and then eluted with acetone and gave a basic material,which by thin-layer chromatography showed the presence of two alkaloids,both reacting positively to alkaloid specific Ehrlich's reagent.The basic material was redissolved with 1% hydrochloric acid and defatted with chlorofrom.The aqua phase was adjusted to pH 10 and successively extracted with chloroform.When the solvent was recovery under reduce condition,the remaining was redissolved with petroleum ether,filtered,concentrated,obtained chief alkaloids form which two alkaloid crystals were separated by chromatography using dry silica gel,eluting with chloroform.